CN107473742B - High-quality single-phase double perovskite Sr2FeMoO6Method for producing ceramic - Google Patents

High-quality single-phase double perovskite Sr2FeMoO6Method for producing ceramic Download PDF

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CN107473742B
CN107473742B CN201710803595.8A CN201710803595A CN107473742B CN 107473742 B CN107473742 B CN 107473742B CN 201710803595 A CN201710803595 A CN 201710803595A CN 107473742 B CN107473742 B CN 107473742B
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王金凤
庄照通
石腾飞
刘帅帅
高迁迁
贾兆静
胡灵活
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Henan Normal University
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Abstract

The invention discloses high-quality single-phase double perovskite Sr2FeMoO6Ceramic materialThe preparation method of the perovskite Sr composite material can obtain high-quality single-phase double perovskite Sr by using a method that a powder mixture is used for embedding a round flake sample in a sintering process and a round open corundum crucible is used for reversely covering the round flake sample under specific and same conditions2FeMoO6The method also has universality for effectively inhibiting volatilization of other volatile components in the double perovskite oxide at high temperature, and the method has simple required equipment and preparation process and better application prospect.

Description

High-quality single-phase double perovskite Sr2FeMoO6Method for producing ceramic
Technical Field
The present invention belongs to double perovskite Sr2FeMoO6The technical field of ceramic synthesis, in particular to high-quality single-phase double perovskite Sr2FeMoO6A method for preparing ceramics.
Background
As early as 50 s in the 20 th century, related to A2B’B’’O6The synthesis and physical studies of perovskite-type double oxides have been reported, and the perovskite-type double oxides are widely concerned due to the unique structure and magnetoelectric properties and the potential application in the aspect of magnetic storage. As A2B’B’’O6Semi-metallic material Sr, one of the representative materials of type double perovskite oxides2FeMoO6Because of having higher Curie temperature (Tc) and excellent room temperature Magnetoresistance (MR), the method has wide application prospect in the aspects of spintronic devices, scientific research and the like, and high-quality Sr is synthesized2FeMoO6The ceramic provides a guarantee for theoretical research and application. But is currently in Sr2FeMoO6During the synthesis of ceramics, Mo often volatilizes at high temperatureInfluence the Fe/Mo ratio and consequently influence the high-quality Sr2FeMoO6And (4) synthesizing the ceramic. In order to solve the problem, in the existing report, the content of Mo is increased in the original proportioning process by a compensation method, but some uncertainty factors exist due to the fact that the content of Mo is increased. Therefore, the Sr capable of effectively inhibiting the double perovskite is designed2FeMoO6High-temperature Mo volatilization of ceramic to prepare high-quality single-phase double perovskite Sr2FeMoO6The ceramic method is particularly important.
Disclosure of Invention
Aiming at the problem that the prior art can not effectively inhibit the double perovskite Sr2FeMoO6The problem of high-temperature Mo volatilization of the ceramic is solved, and the high-quality single-phase double perovskite Sr is provided2FeMoO6A method for preparing ceramics.
The invention adopts the following technical scheme to solve the technical problems, and the high-quality single-phase double perovskite Sr2FeMoO6The preparation method of the ceramic is characterized by comprising the following specific steps:
(1) according to the chemical formula Sr2FeMoO6SrCO with a purity of 99.5% after drying was weighed3Powder, 99.9% purity Fe2O3Powder and MoO with a purity of 99.9%3Adding the mixture of the three kinds of powder into alcohol, and performing ball milling treatment to uniformly mix the powder;
(2) drying the powder mixture obtained in the step (1), grinding and uniformly mixing the powder mixture by using an agate mortar, pre-burning the powder mixture in air of 1173K for 10 hours, and then grinding and uniformly mixing the powder mixture by using the agate mortar;
(3) adding alcohol into the powder mixture obtained in the step (2), performing ball milling treatment to uniformly mix the powder, and then drying;
(4) pressing the powder mixture obtained in the step (3) into a round slice with the diameter of 10mm +/-1 mm and the thickness of 1mm +/-0.1 mm by using the pressure of 4 MPa;
(5) laying the powder mixture obtained in the step (3) in a rectangular open corundum crucible, placing the round slice obtained in the step (4) on the powder mixture, covering the round slice with the powder mixture obtained in the step (3) to embed the round slice into the powder mixture, and finally, using the round open corundum crucible to reversely buckle on the round slice and completely cover the round slice;
(6) placing a rectangular open corundum crucible into a muffle furnace, and introducing flowing H with the volume ratio of 1:92The gas flow of the/Ar mixed protective gas is 20m L/min, the heating rate is 5 ℃/min, in the heating process, the temperature is kept for 30min when the temperature is 673K, then the temperature is raised to 1473K, the sintering temperature is maintained to 1473K, the gas flow is 20m L/min, the sintering time is 40h, and finally the high-quality single-phase Sr is prepared2FeMoO6A ceramic.
Compared with the prior art, the invention has the following beneficial effects: the equipment and the preparation process required by the invention are simple, and the high-quality single-phase double perovskite Sr can be obtained by the method of embedding the sample round slice by using the powder mixture and completely covering the sample round slice by using the round open corundum crucible in a reverse buckling manner in the sintering process under the specific and same conditions2FeMoO6Ceramics, and the method also has universality for effectively inhibiting volatilization of other volatile components in the double perovskite oxide at high temperature.
Drawings
FIG. 1 shows two Sr portions obtained in example2FeMoO6XRD pattern of the ceramic.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
(1) According to the chemical formula Sr2FeMoO6Weighing the dried SrCO3(99.5%) powder, Fe2O3(99.9%) powder and MoO3(99.9%) powder, adding the mixture of the three powders into alcohol, and performing ball milling treatment (320 r/min, 24 h) to uniformly mix the powders;
(2) drying the powder mixture obtained in the step (1), grinding the powder mixture uniformly by using an agate mortar, pre-burning the powder mixture in air of 1173K for 10 hours, and grinding the powder mixture uniformly by using the agate mortar;
(3) adding the powder mixture obtained in the step (2) into alcohol, performing ball milling treatment (320 r/min, 24 h) to uniformly mix the powder, and then drying;
(4) pressing the powder mixture obtained in the step (3) into a round slice with the diameter of 10mm +/-1 mm and the thickness of 1mm +/-0.1 mm by using the pressure of 4 MPa;
(5) laying the powder mixture obtained in the step (3) in a rectangular open corundum crucible, placing the round slice obtained in the step (4) on the powder mixture, and covering the round slice with the powder mixture obtained in the step (3) to enable the round slice to be embedded in the powder mixture;
(6) placing a rectangular open corundum crucible into a muffle furnace, and introducing flowing H with the volume ratio of 1:92The gas flow rate of the/Ar mixed protective gas is 20m L/min, the heating rate is 5 ℃/min, in the heating process, the temperature is kept for 30min when the temperature is 673K, then the temperature is raised to 1473K, the sintering temperature is maintained to 1473K, the gas flow rate is 20m L/min, the sintering time is 40h, and finally the Sr is prepared2FeMoO6A ceramic.
Example 2
The other reaction conditions were the same as in example 1, with the following changes: embedding Sr with powder mixture during sintering2FeMoO6Sheet sample and fully covered Sr with a round open corundum crucible upside down2FeMoO6The method of the thin slice sample can obtain high-quality single-phase Sr2FeMoO6A ceramic.
And (3) testing results:
FIG. 1 shows the two Sr portions obtained2FeMoO6X-ray diffraction (XRD) contrast of ceramics, S1 shows a single-phase Sr as a main diffraction peak2FeMoO6However, diffraction peaks for the hetero-phase Fe are clearly present, as indicated by the grey boxes. The absence of the diffraction peak of this hetero-phase Fe in S2 indicates thatSr prepared under the condition2FeMoO6The ceramic is a high quality single phase.
While there have been shown and described what are at present considered the fundamental principles of the invention, its essential features and advantages, the invention further resides in various changes and modifications which fall within the scope of the invention as claimed.

Claims (1)

1. High-quality single-phase double perovskite Sr2FeMoO6The preparation method of the ceramic is characterized by comprising the following specific steps:
(1) according to the chemical formula Sr2FeMoO6SrCO with a purity of 99.5% after drying was weighed3Powder, 99.9% purity Fe2O3Powder and MoO with a purity of 99.9%3Adding the mixture of the three kinds of powder into alcohol, and performing ball milling treatment to uniformly mix the powder;
(2) drying the powder mixture obtained in the step (1), grinding and uniformly mixing the powder mixture by using an agate mortar, pre-burning the powder mixture in air of 1173K for 10 hours, and then grinding and uniformly mixing the powder mixture by using the agate mortar;
(3) adding alcohol into the powder mixture obtained in the step (2), performing ball milling treatment to uniformly mix the powder, and then drying;
(4) pressing the powder mixture obtained in the step (3) into a round slice with the diameter of 10mm +/-1 mm and the thickness of 1mm +/-0.1 mm by using the pressure of 4 MPa;
(5) laying the powder mixture obtained in the step (3) in a rectangular open corundum crucible, placing the round slice obtained in the step (4) on the powder mixture, covering the round slice with the powder mixture obtained in the step (3) to embed the round slice into the powder mixture, and finally, using the round open corundum crucible to reversely buckle on the round slice and completely cover the round slice;
(6) placing a rectangular open corundum crucible into a muffle furnace, and introducing flowing H with the volume ratio of 1:92The flow rate of the gas is 20m L/min, the heating rate is 5 ℃/min, and the temperature is 673K in the heating processKeeping the temperature for 30min, then heating to 1473K, keeping the sintering temperature at 1473K and the gas flow at 20m L/min, and sintering for 40h to obtain the high-quality single-phase Sr2FeMoO6A ceramic.
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CN112125341A (en) * 2020-09-23 2020-12-25 齐齐哈尔大学 Double perovskite type semi-metallic material and preparation method thereof
CN112331435B (en) * 2020-10-09 2024-01-19 河南师范大学 Sr 2 FeMoO 6 (1-x)-CoFe 2 O 4 (x) Method for regulating and controlling magnetic resistance conversion behavior of composite material

Citations (2)

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Publication number Priority date Publication date Assignee Title
CN102633495A (en) * 2012-04-11 2012-08-15 南京大学 Preparation method of room-temperature ferromagnetic Sr2FemMonO6 ceramic
CN103193487A (en) * 2013-04-22 2013-07-10 南京大学 Method for quantitatively controlling B-position antiposition defect concentration of Sr2FeMoO6 ceramic

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102633495A (en) * 2012-04-11 2012-08-15 南京大学 Preparation method of room-temperature ferromagnetic Sr2FemMonO6 ceramic
CN103193487A (en) * 2013-04-22 2013-07-10 南京大学 Method for quantitatively controlling B-position antiposition defect concentration of Sr2FeMoO6 ceramic

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